반응 #345990

반응 방정식

para-methylphenethylamine

benzene

ortho-methoxyphenol

formalin

→

8-methoxy-3-(4-methylphenethyl)-3,4-dihydro-2H-1,3-benzoxazine

반응 조건

후처리

1. 1
   온도The mixture is heated
2. 2
   온도on reflux for 10 hours
3. 3
   농축concentrated to dryness under reduced pressure
4. 4
   기타The residue is purified by column chromatography on silica gel with a mixture of acetone and benzene (1:4)
5. 5
   workup.WAITThe resultant oil is left
6. 6
   온도at cool place for a week
7. 7
   기타Recrystallization from normal hexane

실험 절차

To 20 ml. of benzene are added 5g. of ortho-methoxyphenol, 9ml. of 37 % formalin and 6.5 g. of para-methylphenethylamine. The mixture is heated on reflux for 10 hours and concentrated to dryness under reduced pressure. The residue is purified by column chromatography on silica gel with a mixture of acetone and benzene (1:4). The resultant oil is left standing at cool place for a week to be solidified. Recrystallization from normal hexane yields 8-methoxy-3-(4-methylphenethyl)-3,4-dihydro-2H-1,3-benzoxazine as colorless needles melting at 58°-63° C. Yield: 1.2 g.

출처